CN109959645B - Method and device for evaluating coating completeness of lithium ion battery shell and core structure material - Google Patents
Method and device for evaluating coating completeness of lithium ion battery shell and core structure material Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/041—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method and a device for evaluating the coating completeness of a shell-core structure material of a lithium ion battery. The evaluation method comprises the following steps: respectively carrying out Raman spectrum detection and conductivity detection on the shell-core structure material; and obtaining the evaluation result of the coating completeness of the shell-core structure material according to the results of the Raman spectrum detection and the conductivity detection. The method adopts conventional macroscopic characterization means, is convenient to measure, can quickly obtain an accurate result, comprehensively and accurately judge the coating completeness of the electrode material, and also verifies the accuracy through electrochemical tests. The method is rapid and efficient, the obtained result is accurate and convenient, the electrochemical performance of the material can be accurately and preliminarily predicted, meanwhile, excellent products are screened out, the inferior-quality products are removed, subsequent meaningless tests are saved, the cost of the test research and development period of the material is remarkably shortened, the efficiency is improved, and the method has important significance for the screening research and development tests of the battery material.
Description
Technical Field
The invention relates to the field of material detection, in particular to a method for evaluating the coating completeness of a shell-core structure material of a lithium ion battery.
Background
Since the advent of lithium ion batteries, lithium ion batteries have been rapidly developed in recent years due to their advantages of high energy density, high average output voltage, small self-discharge, high safety, and the like. With the wide application of lithium ion batteries, the requirements on battery systems are higher and higher, and battery systems with high energy density and safety become hot spots.
Among the components of the battery system, the battery material is undoubtedly the most critical one, since the main body of the charge-discharge reaction is the battery material, whose electrochemical reaction characteristics determine the upper limit of the battery material. Therefore, much attention has been paid to the development of new battery materials. After the battery material is researched and prepared, the performance of the battery is evaluated, and the fact that a test result can be fed back in time is also a key part in the whole process. Among the novel electrode materials, high-capacity alloy-like negative electrode materials, such as Si and the like, are ideal choices for realizing a new generation of high-energy-density batteries. However, in the actual process, if such materials are not processed, due to the volume expansion effect caused by the alloy reaction, the SEI can thicken and separate from the current collector, and other adverse effects can be caused, so that the capacity is rapidly attenuated, and the cyclicity is poor, which is also a problem that needs to be solved urgently by such materials.
In order to solve the adverse effect caused by volume expansion, the most popular strategy in recent years is to perform coating treatment on the outside of an alloy material, and inhibit the volume effect of an internal active substance by utilizing the low volume expansion rate and the mechanical and chemical stability of the coating material so as to achieve the aim of improving the electrochemical performance. In this process, the quality of the coating becomes critical. The coating completeness is a key index, if the coating is incomplete, the buffer characteristic of the coating material cannot be fully exerted, and meanwhile, the contact between the electrolyte and the internal active substance cannot be fully prevented, so that the overall performance is affected. The existing methods detect coating completeness mainly by microscopic characterization means, such as high-resolution TEM. Microscopic characterization, because of the small field of view, only a single particle can be seen at high magnification, and although accurate, the overall efficiency is low, and the coating state of multiple particles cannot be reflected. Meanwhile, TEM is adopted for representing and sample preparation, the requirement is high, the conditions of solvent and ultrasonic dispersion are strictly controlled, if the treatment is careless in the links, the structure of the particles can be damaged, the observation accuracy is affected, the process is complex, and the efficiency is low. Therefore, the cladding completeness is checked by a simple, convenient and effective macroscopic characterization means, the accuracy is ensured, the integral cladding state can be reflected, and the method has important significance for shortening the test research and development cycle cost of the whole material, improving the efficiency and screening, research and development tests.
Disclosure of Invention
The invention aims to provide an evaluation method for coating completeness of a lithium ion battery shell-core structure material, which aims to solve the problem that only a microscopic representation means can be adopted in the existing battery material coating inspection, has the advantages of ensuring the accuracy, being simple, convenient and efficient, reflecting the overall coating state of the material, shortening the overall research and development period and improving the screening efficiency of excellent and defective products. In addition, the invention also provides a device for evaluating the coating completeness of the shell-core structure material of the lithium ion battery. The following presents a simplified summary in order to provide a basic understanding of some aspects of the disclosed embodiments. This summary is not an extensive overview and is intended to neither identify key/critical elements nor delineate the scope of such embodiments. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is presented later.
First, some technical terms appearing herein are explained.
The shell-core structure material refers to a composite material which can be applied to an electrode material of a lithium ion battery, particularly a negative electrode material, and has the shell-core structure characteristic. The shell-core structure material is formed by compounding an inner layer and an outer layer, the inner layer and the outer layer are made of different materials, and the outer layer is coated on the inner layer. It is noted that the structure of the core-shell structure material herein may be a double-layer structure, such as Si @ C, with an inner layer of Si and an outer layer of C; the structure of the shell-core structure material can also be a composite structure with more than three layers, such as Si @ C @ TiO2For this class of materials, the inner layer is then Si @ C and the outer layer is the outermost layer of TiO coated with Si @ C2。
The coating completeness refers to an evaluation parameter of the coating state of an outer layer to an inner layer in the shell-core structure material. In the prior art, the macroscopic test method for the coating degree or the coating rate is generally determined by determining the mass of an inner layer and an outer layer and then determining the mass ratio, although the overall proportion of an outer layer material in a shell-core structure material can be effectively determined by the method, whether the outer layer material is completely coated on the inner layer material cannot be accurately determined, whether the surface of the inner layer material is completely coated is an important index influencing an electrode material in the field of batteries, the coating completeness is a key index, if the coating is incomplete, the buffer characteristic of the coating material cannot be fully exerted, and meanwhile, the contact between an electrolyte and an internal active substance cannot be fully prevented, so that the overall performance is influenced. As mentioned above, the microscopic characterization means commonly used in the prior art, such as high-resolution TEM, can only see a single particle due to the small field of view, and is accurate but inefficient as a whole, and cannot reflect the coating state of multiple particles.
The exposure index E is an important index for quantitatively measuring the completeness of the coating layer in the core-shell structural material and is calculated according to Raman spectrum data of the core-shell structural material, the exposure index E represents an index of the exposure of an inner layer, and the exposure index E and the completeness of the coating are in a negative correlation relationship.
The characteristic component refers to a specific component in the inner layer or the outer layer of the shell-core structure material, and can be used for marking the layer with characteristics. The first characteristic component is used for marking the inner layer of the shell-core structural material, and the second characteristic component is used for marking the outer layer of the shell-core structural material. The first characteristic peak is at least one characteristic peak of the first characteristic component, the second characteristic peak is at least one characteristic peak of the second characteristic component, and the selection of the characteristic peaks needs to be determined according to factors such as sensitivity, intensity and interference degree of the characteristic peaks.
The evaluation strategy is preset to determine the coating completeness of the core-shell material based on the exposure index E and the conductivity. The presentation mode of the evaluation strategy can be flexibly set according to needs, and the coating completeness can be determined through the exposure index E and the conductivity by utilizing a mathematical model constructed by the exposure index E and the conductivity. The coating completeness of the core-shell structure material corresponding to the exposure index E and the conductivity can also be determined by means of a table look-up.
The evaluation result refers to the evaluation of the coating completeness of the shell-core structure material, and the specific mode is not particularly limited, and specifically may be a class of grade indexes such as "excellent, good, medium, poor", "first-class, second-class, and third-class".
The present invention will be specifically explained below.
The invention aims to provide a method for evaluating the coating completeness of a shell-core structure material of a lithium ion battery.
In some exemplary embodiments, the evaluation method includes:
respectively carrying out Raman spectrum detection and conductivity detection on the shell-core structure material;
and obtaining the evaluation result of the coating completeness of the shell-core structure material according to the results of the Raman spectrum detection and the conductivity detection.
In the above embodiment, the Raman mapping may comprise:
determining a proper detection wavelength according to the material information of the shell-core structure material;
performing Raman test on the shell-core structure material under the detection wavelength to obtain a Raman spectrum of the shell-core structure material;
the material information refers to information capable of representing material components and structural characteristics, and the detection wavelength suitable for Raman detection can be determined according to the information.
The conductivity detection is an operation of obtaining the conductivity of the shell-core structure material, and can be a step of sending a detection instruction to detection equipment in a communication mode so as to obtain a detection result; or generating a detection signal inside the system, and performing conductivity test inside the system according to the detection signal to further obtain a detection result.
The completeness of coating needs to be determined simultaneously according to the results of Raman spectrum detection and conductivity detection. Although both Raman spectrum and conductivity are evaluation indexes of coating completeness of the shell-core structure material, the indexes cannot be used for evaluating the coating completeness alone. Wherein, the detection result of the Raman spectrum represents the exposure degree of the inner layer on the whole shell-core structural material, and the conductivity represents the electric property of the whole shell-core structural material. In a specific evaluation process, the coating completeness needs to be evaluated simultaneously by combining the two parameters, so that the evaluation accuracy is further improved.
The above embodiment provides a novel method for testing the coating completeness of the shell-core structure material in the battery field. And the coating completeness of the material is evaluated by using Raman spectrum test and conductivity test, so that the method is simple, convenient and effective. The evaluation of the coating completeness of the shell-core structure material in the battery field has important significance, for example, although the prior art has more reports about the development results of the shell-core structure material of the battery, a macro characterization method which is rapid and effective for the coating quality, namely the coating completeness, of the material is lacked. The embodiment solves the problems and has important significance for the industrial application of the shell-core structure material in the field of batteries.
Optionally, the Raman mapping comprises:
obtaining a Raman spectrum of the shell-core structure material;
and analyzing the Raman spectrum of the core-shell structure material to determine the exposure index E.
Further, the exposure index E corresponds to the coating completeness of the inner layer by the outer layer; the operation of analyzing the Raman spectrum of the core-shell structure material and determining the exposure index E specifically comprises the following steps:
extracting the intensity of at least one characteristic peak of each characteristic component from the Raman spectrum of the core-shell structure material according to the at least one characteristic component of the inner layer and the outer layer respectively;
calculating the exposure index E based on the intensity of at least one characteristic peak of each of the characteristic components.
The above embodiment provides a specific way to determine the exposure index E, and in a specific implementation process, it is necessary to determine characteristic components and corresponding characteristic peaks that can perform characteristic marking on the inner layer and the outer layer according to the characteristics of the materials of the inner layer and the outer layer, and the types and amounts of the characteristic components can be comprehensively determined according to the characteristics of elements in the materials and the characteristics of peaks of the elements in the Raman spectrum. Then, the intensities of characteristic peaks corresponding to the characteristic components are extracted from the Raman spectrum, and the exposure index E is calculated from the intensities of the characteristic peaks. The embodiment provides a specific method for determining the exposure index, and the accuracy of the exposure index E is further improved.
The following examples present preferred modes of the above-described embodiments.
Preferably, the inner layer of the core-shell structural material contains a first characteristic component, and the outer layer contains a second characteristic component; extracting the intensity of a first characteristic peak corresponding to the first characteristic component, and extracting the intensity of a second characteristic peak corresponding to the second characteristic component;
said operation of calculating said exposure index E based on the intensity of at least one characteristic peak of each of said characteristic components comprises:
and calculating the ratio of the intensities of the first characteristic peak and the second characteristic peak according to the intensity of the first characteristic peak and the intensity of the second characteristic peak, and outputting the ratio as the exposure index E.
Optionally, the evaluation result of the coating completeness of the shell-core structural material is obtained according to the exposure index E, the conductivity of the shell-core structural material, and a preset evaluation strategy, and the process specifically includes:
determining a first evaluation result of the coating completeness of the shell-core structural material corresponding to the value of the exposure index E according to the evaluation strategy and the exposure index E;
determining a second evaluation result of the coating completeness of the shell-core structural material corresponding to the value of the conductivity of the shell-core structural material according to the evaluation strategy and the conductivity of the shell-core structural material;
and if the first evaluation result is consistent with the second evaluation result, outputting the evaluation result as the evaluation result of the coating completeness of the shell-core structure material.
And if the first evaluation result is inconsistent with the second evaluation result, outputting the exposure index E, the conductivity of the shell-core structure material and an evaluation report corresponding to the parameters.
The above example shows a preferred embodiment of how the completeness of the coating of a core-shell structured material can be assessed in terms of exposure index E and conductivity. In the embodiment, firstly, the evaluation results corresponding to the parameter values are obtained according to the exposure index E and the conductivity, then whether the two evaluation results are consistent or not is judged, if so, the correctness of the evaluation is verified, and then the evaluation results are output. And if the two are not consistent, generating the evaluation report. The accuracy of the evaluation result is further improved, and the user experience is improved.
Taking a specific embodiment of the core-shell structure material as follows, if the core-shell structure material is silicon Si @ carbon C, the first characteristic component is Si, and the second characteristic component is C; obtaining the wave number of Si at 500cm according to the Raman spectrum of the Si @ C-1The peak intensity of C at a wave number of 1580cm-1(ii) peak intensity of; the exposure index E is the index Si is at 500cm-1(ii) peak intensity of (D) and said C at wave number of 1580cm-1The smaller the value of the exposure index E, the higher the coating completeness of the core-shell structured material.
The embodiment provides a preferable embodiment for evaluating the coating completeness of a negative electrode material Si @ C in the field of batteries, and discloses a selection method of a characteristic component, a selection method of a characteristic peak and a calculation method of an exposure index E. In the Raman spectrum obtained, it is preferable to obtain Si at 500cm-1Peak intensity of (C) at 1300cm-1Intensity of peak D of (2) and 1580cm-1G peak intensity of (a). The exposure index, E-index, in this example is the ratio of the peak intensity of Si to the peak intensity of G for C. If the coating is completely uniform and the internal Si is not exposed, the Si does not peak, and E is 0; if the more incomplete the coating and the more exposed the Si inside, the higher the Si peak intensity, and the larger E. According to the method for evaluating the coating completeness of Si @ C disclosed by the embodiment, the Si @ C can be quickly and effectively detected, the accuracy is ensured, the integral coating state can be reflected, and the method has important significance for shortening the test research and development period cost of the whole material, improving the efficiency and screening, research and development tests.
Optionally, before performing the Raman spectrum detection and the conductivity detection, the method further includes:
purifying the shell-core structure material to remove impurities in the shell-core structure material.
Considering that the battery material may contain impurities, the shell-core structure material can be purified before the evaluation method is carried out, and the accuracy and the effectiveness of the evaluation method are further improved.
The above evaluation method will be described below with reference to a specific embodiment.
In some specific embodiments, the method for evaluating the coating completeness of the lithium ion battery shell and core structure material comprises the following steps:
1) raman spectrum detection: detecting the Raman spectrum of the sample under a certain wavelength, and calculating an exposure index E;
2) and (3) detecting the conductivity of the powder: putting the lithium ion battery shell and core structure material powder into a test bench for pressurization test to obtain a conductivity value under a certain pressure;
3) and determining corresponding evaluation results according to the exposure index E and the conductivity, and outputting the results if the evaluation results of the exposure index E and the conductivity are consistent.
Specifically, the Raman spectrum detection comprises the following steps:
taking a proper amount of powder to be detected to a clean glass slide;
testing at a proper wavelength to obtain a Raman spectrum;
the exposure index E is calculated.
Further, the powder conductivity detection comprises the following steps:
taking a proper amount of powder to be detected and putting the powder into a test bench for testing the powder conductivity;
a compression test was performed. When the powder is pressed to a certain pressure, the display table has a numerical value, and the powder is just compacted to a measurable range. At this time, the critical tabletting pressure of the powder is tested, and the powder needs to be continuously pressurized to the critical tabletting pressure of at least 2-3Mpa, so that the test accuracy is ensured. Since conductivity increases with increasing pressure above the critical sheeting pressure, bulk conductivity values for samples of the same system are obtained at the same pressure for comparison purposes.
Another objective of the present invention is to provide a device for testing the coating completeness of the lithium ion battery shell and core structure material.
In some exemplary embodiments, the test device includes:
the first testing unit is used for carrying out Raman spectrum detection on the shell-core structure material;
the second test unit is used for detecting the conductivity of the shell-core structure material;
and the evaluation unit is used for acquiring the evaluation result of the coating completeness of the shell-core structure material according to the detection results of the first test unit and the second test unit.
In some optional embodiments, the second test unit comprises:
the acquisition unit is used for acquiring a Raman spectrum of the shell-core structure material;
and the analysis unit is used for analyzing the Raman spectrum of the core-shell structure material and determining the exposure index E.
In some alternative embodiments, the core-shell structural material comprises an inner layer and an outer layer, the exposure index E corresponding to the completeness of coating of the inner layer by the outer layer; the analysis unit includes:
an extraction unit, which is used for extracting the intensity of at least one characteristic peak of each characteristic component from the Raman spectrum of the shell-core structure material according to the at least one characteristic component of the inner layer and the outer layer;
and the calculation unit is used for calculating the exposure index E according to the intensity of at least one characteristic peak of each characteristic component.
In some alternative embodiments, the inner layer of the core-shell structural material contains a first characteristic component and the outer layer contains a second characteristic component; the extraction unit includes:
a first extraction subunit configured to extract an intensity of a first characteristic peak corresponding to the first characteristic component;
a second extraction subunit operable to extract an intensity of a second characteristic peak corresponding to the second characteristic component;
the calculation unit includes:
and a calculating subunit, configured to calculate, based on the intensity of the first characteristic peak and the intensity of the second characteristic peak, a ratio of the intensities of the first characteristic peak and the second characteristic peak, which is output as the exposure index E.
In some optional embodiments, the evaluation unit comprises:
a first evaluation subunit, configured to determine, according to the evaluation strategy and the exposure index E, a first evaluation result of the coating completeness of the core-shell structural material corresponding to the value of the exposure index E;
a second evaluation subunit, configured to determine, according to the evaluation strategy and the electrical conductivity of the shell-core structure material, a second evaluation result of the coating completeness of the shell-core structure material corresponding to the value of the electrical conductivity of the shell-core structure material;
and a judging unit for comparing the first evaluation result with the second evaluation result, and outputting the evaluation result as an evaluation result of the coating completeness of the core-shell structure material if the first evaluation result is consistent with the second evaluation result.
In some alternative embodiments, the core-shell structure material is Si @ C, the first characteristic component is Si, and the second characteristic component is C; the first evaluation subunit respectively acquires Si with wave number of 500cm according to the Raman spectrum of the Si @ C-1The peak intensity of C at a wave number of 1580cm-1(ii) peak intensity of; the exposure index E is that the Si is 500cm-1(ii) peak intensity of (D) and said C at wave number of 1580cm-1The smaller the value of the exposure index E, the higher the coating completeness of the core-shell structured material.
Compared with the prior art, the invention has the following advantages and improvement effects:
1) the adopted methods are all conventional macroscopic characterization methods, the measurement is convenient, and the result can be obtained quickly.
2) The coating state of the entire material can be reflected.
3) The Raman spectrum defines an exposure index E which can be used as an important index for quantitatively measuring the completeness of the coating layer.
4) The comprehensive characterization result can more accurately judge the coating completeness of the electrode material, and the accuracy of the method is verified through electrochemical tests.
5) The method can accurately and preliminarily predict the electrochemical performance of the material, simultaneously screen out excellent products to remove inferior-quality products, save subsequent meaningless tests, remarkably shorten the cost of the test research and development period of the material, and remarkably improve the efficiency.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
Fig. 1 is a schematic flow chart of a method for evaluating coating completeness of a lithium ion battery shell-core structure material according to an embodiment of the present invention.
Fig. 2 is a schematic flow chart of a method for evaluating the coating completeness of a lithium ion battery shell-core structure material according to an embodiment of the present invention.
FIG. 3 is a schematic flow chart of a coating completeness evaluation method of Si @ C according to an embodiment of the invention.
FIG. 4 is a Raman spectrum of three samples in different coating states in an example of the present invention.
FIG. 5 is a graph showing the cycle performance of three samples of different coating states in an example of the present invention.
Fig. 6 is a block diagram of a testing apparatus 600 for completeness of coating of a core structure material of a lithium ion battery in an embodiment of the present invention.
Fig. 7 is a block diagram of a testing apparatus 700 for testing the completeness of coating of a core structure material of a lithium ion battery in an embodiment of the present invention.
Detailed Description
The following description and the drawings sufficiently illustrate specific embodiments of the invention to enable those skilled in the art to practice them. The examples merely typify possible variations. Individual components and functions are optional unless explicitly required, and the sequence of operations may vary. Portions and features of some embodiments may be included in or substituted for those of others. The scope of embodiments of the invention encompasses the full ambit of the claims, as well as all available equivalents of the claims. Embodiments may be referred to herein, individually or collectively, by the term "invention" merely for convenience and without intending to voluntarily limit the scope of this application to any single invention or inventive concept if more than one is in fact disclosed. Herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed. The embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the structures, products and the like disclosed by the embodiments, the description is relatively simple because the structures, the products and the like correspond to the parts disclosed by the embodiments, and the relevant parts can be just described by referring to the method part.
Fig. 1 is a schematic flow chart illustrating a method for evaluating the coating completeness of a lithium ion battery shell and core structure material according to an exemplary embodiment, where as shown in fig. 1, the process of the method for evaluating the coating completeness of the lithium ion battery shell and core structure material includes:
step 101, performing Raman spectrum detection and conductivity detection on the shell-core structure material respectively;
and step 102, obtaining an evaluation result of the coating completeness of the shell-core structure material according to the results of the Raman spectrum detection and the conductivity detection.
Wherein, in step 101, the Raman mapping comprises:
obtaining a Raman spectrum of the shell-core structure material;
analyzing the Raman spectrum of the shell-core structure material to determine an exposure index E;
in step 102, the obtaining of the evaluation result of the coating completeness of the shell-core structure material includes:
and determining the evaluation result of the coating completeness of the shell-core structure material according to the exposure index E and the conductivity.
Further, the core-shell structure material comprises an inner layer and an outer layer, and the exposure index E corresponds to the coating completeness of the inner layer by the outer layer. The operation of determining the exposure index E comprises:
extracting the intensity of at least one characteristic peak of each characteristic component from the Raman spectrum of the core-shell structure material according to the at least one characteristic component of the inner layer and the outer layer respectively;
calculating the exposure index E based on the intensity of at least one characteristic peak of each of the characteristic components.
The above-described flow is incorporated into specific embodiments below. Fig. 2 is a schematic flow chart of a method for evaluating the coating completeness of a lithium ion battery shell-core structure material according to an embodiment of the present invention. The inner layer of the core-shell structural material contains a first characteristic component, and the outer layer contains a second characteristic component; the first characteristic peak corresponds to the first characteristic component, and the second characteristic peak corresponds to the second characteristic component. As shown in fig. 2, the evaluation method includes:
step 201, Raman spectrum detection;
obtaining a Raman spectrum of the shell-core structure material;
step 202, extracting the intensities of the first characteristic peak and the second characteristic peak;
extracting the intensity of a first characteristic peak corresponding to the first characteristic component, and extracting the intensity of a second characteristic peak corresponding to the second characteristic component;
step 203, calculating an exposure index E;
calculating a ratio of the intensities of the first characteristic peak and the second characteristic peak from the intensities of the first characteristic peak and the second characteristic peak, which is output as the exposure index E;
step 204, determining a first evaluation result according to the exposure index E;
determining a first evaluation result of the coating completeness of the shell-core structural material corresponding to the value of the exposure index E according to the evaluation strategy and the exposure index E;
step 205, detecting the conductivity of the shell-core structure material;
step 206, determining a second evaluation result according to the conductivity;
determining a second evaluation result of the coating completeness of the shell-core structural material corresponding to the value of the conductivity of the shell-core structural material according to the evaluation strategy and the conductivity of the shell-core structural material;
step 207, comparing and outputting the evaluation results;
and if the first evaluation result is consistent with the second evaluation result, outputting the evaluation result as the evaluation result of the coating completeness of the shell-core structure material.
In the above flow, if the core-shell structure material is silicon Si @ carbon C, the first characteristic component is Si, and the second characteristic component is C; testing at the wavelength of He-Ne 632nm to obtain Raman spectrum; obtaining the wave number of Si at 500cm according to the Raman spectrum of the Si @ C-1The peak intensity of C at a wave number of 1580cm-1(ii) peak intensity of; the exposure index E is that the Si is 500cm-1Has a peak intensity of 1580cm in wave number with C-1The smaller the value of the exposure index E, the higher the coating completeness of the core-shell structured material.
Further, before step 201, a purification operation is further included, which is used to purify the core-shell structured material to remove impurities in the core-shell structured material.
Next, a method for evaluating the coating completeness of Si @ C will be described by way of example according to a specific embodiment; the detection devices used in the present embodiment are all commonly used characterization devices, and the reagents used in the battery performance test are also commonly used battery grade reagents, which are all commercially available. The whole detection process uses no special characterization equipment or reagent. As shown in fig. 3, the method for evaluating the coating completeness of Si @ C includes:
step 301, obtaining a Raman spectrum;
firstly, taking a proper amount of powder to a clean glass slide, and then testing under the wavelength of He-Ne 632nm to obtain a Raman spectrum;
step 302, calculating an exposure index E;
obtaining Si at a wavenumber of 500cm-1The peak intensity of C at a wave number of 1580cm-1(ii) peak intensity of; the exposure index E is that the Si is 500cm-1Has a peak intensity of 1580cm in wave number with C-1The ratio of peak intensities of (a);
step 303, detecting the conductivity of the powder;
and (3) putting a proper amount of powder to be detected into a test bench for testing the powder conductivity, and performing tabletting test, wherein when the pressure is increased to 5Mpa, the test bench has a numerical value, and the critical tabletting pressure of the Si @ C powder is tested. In order to ensure the accuracy of the test and conveniently compare and pressurize to 10Mpa to obtain the value of the conductivity of the body under the pressure.
Step 304, determining a first evaluation result according to the exposure index E;
the Si @ C evaluation strategy can determine an evaluation result corresponding to the numerical value of the exposure index E in a table look-up mode; the Si @ C evaluation strategy is preset in a memory, and the evaluation strategy records the numerical ranges of the exposure index E and the conductivity and corresponding evaluation results respectively;
in particular, for Si @ C powders, the evaluation strategy can be as follows:
TABLE 1 Si @ C powder coating completeness evaluation strategy
| Completeness of coating | Exposure index E | Conductivity (omega cm)-1) |
| >80％ | <0.2 | <0.5 |
| 60～80％ | 0.2～0.4 | 0.5～1 |
| 40～60％ | 0.4～0.7 | 1～1.5 |
| <40％ | >1 | >2 |
Step 305, determining a second evaluation result according to the conductivity;
approximately, a second evaluation result corresponding to the current conductivity may be determined according to table 1;
step 306, verifying the accuracy of the evaluation result;
and checking whether the first evaluation result is consistent with the second evaluation result, and if so, outputting the evaluation result.
The embodiment provides the evaluation method for the coating completeness of the battery cathode material Si @ C, the Raman spectrum test and the conductivity test are utilized to evaluate the coating completeness of the material, and the evaluation method is simple, convenient and effective and has important significance for the industrial application of the shell-core structure material in the field of batteries. The embodiment discloses a specific implementation method for evaluating the coating completeness of Si @ C, and the method has a guiding function on evaluating the coating completeness of Si @ C.
In order to further verify the technical effect of the method for evaluating the coating completeness of the core-shell structure material in the above embodiment, the method described in the above embodiment is combined with the test results of electrochemical performance to describe the method.
The method for testing the electrochemical performance specifically comprises the following steps:
mixing thickener carboxymethylcellulose sodium (CMC) powder with ultrapure deionized water at a ratio of 1:99 at normal temperature, and stirring at normal temperature for 12h to obtain transparent viscous colloidal solution. According to active substance (Si @ C): conductive agent super P: styrene Butadiene Rubber (SBR) 8: 1: 0.5: adding each component substance according to a mass ratio of 0.5, stirring for 0.5h after adding active substances, stirring for 1.5h after adding conductive agent super P, complementing required amount of solvent ultrapure deionized water to enable the solid content to be 10 wt.%, stirring for 6h, finally adding binder Styrene Butadiene Rubber (SBR), stirring at low speed for 0.5h to enable the solution to be in a transparent black state, and obtaining the cathode slurry. According to the conventional production process of the lithium ion button cell, aqueous negative electrode slurry is coated on a current collector by a wet film preparation method, and a negative electrode plate can be obtained by punching a dry film through punching equipment through drying and dehydrating and deoxidizing processes. And assembling the button half cell with a metal lithium sheet, a diaphragm, electrolyte, a positive and negative electrode shell, a spring sheet and a gasket in a glove box, and standing for 12 hours to obtain the lithium ion button half cell with fully soaked interior.
According to the specific implementation method described in the above embodiment, the coating completeness of three different coating state Si @ C samples A \ B \ C is tested. The following table shows the results of the exposure index E and conductivity and cycling stability for the a/B/C samples:
TABLE 2 Exposure index E and conductivity results and cycling stability for samples in different coating states
| Sample (I) | Exposure index E | Conductivity (omega cm)-1) | Capacity retention (%) |
| A | 0.04 | 0.26 | 87.9 |
| B | 0.32 | 0.35 | 65.1 |
| C | 1.56 | 2.14 | 23.7 |
As can be seen from the data in the table above, the exposure index E correlates with coating completeness. The more complete the coating, the smaller the E index. Meanwhile, the more complete the coating, the more complete the conductive network formed by the coating, and the better the overall conductivity, which is consistent with the result of conductivity. FIG. 4 shows that in the spectrum comparison of Raman spectra of three samples, 500cm-1Peak intensity of Si at 1580cm-1In the case of comparable basic intensity of the G peak at C, the A sample is close to 0 and the C sample is the highest, showing that the A sample is coated the most completely and the C sample is coated the least completely. And the subsequent test results of electrochemical cycling as an active material of the three samples in fig. 5 can verify that the sample a with the highest coating property is most stable in cycling, and shows that the completely coated outer layer can fully protect the inner layer in the electrochemical reaction. In contrast, the C sample with the worst coating performance had the worst cycle performance, indicating that the inner active material was exposed more and the protective effect of the coating layer of the outer layer was greatly impaired when the coating was insufficient. The results of fig. 5 are consistent with fig. 4, the more complete the coating, the better the capacity retention, and the correctness of the method is also verified.
Fig. 6 is a block diagram of a testing apparatus for completeness of coating of a lithium ion battery shell core structure material according to an exemplary embodiment of the present invention. As shown in fig. 6, the testing apparatus 600 includes:
the first testing unit 601 is used for performing Raman spectrum detection on the shell-core structure material;
a second testing unit 602, configured to perform conductivity detection on the core-shell structure material;
an evaluation unit 603, configured to obtain an evaluation result of the coating completeness of the core-shell structure material according to the detection results of the first test unit and the second test unit.
Specifically, the first test unit 601 includes:
an acquiring unit 6011, configured to acquire a Raman spectrum of the core-shell structure material;
an analyzing unit 6012, configured to analyze the Raman spectrum of the core-shell structured material, and determine the exposure index E.
The core-shell structure material comprises an inner layer and an outer layer, and the exposure index E corresponds to the coating completeness of the inner layer by the outer layer.
Optionally, the analysis unit 6012 includes:
an extraction unit 60121, configured to extract an intensity of at least one characteristic peak of each characteristic component from the Raman spectrum of the core-shell structured material according to at least one characteristic component of the inner layer and the outer layer, respectively;
a calculating unit 60122 for calculating the exposure index E based on the intensity of at least one characteristic peak of each of the characteristic components.
Optionally, the inner layer of the core-shell structural material contains a first characteristic component, and the outer layer contains a second characteristic component; the extraction unit 60121 includes:
a first extraction subunit 601211, configured to extract an intensity of a first characteristic peak corresponding to the first characteristic component;
a second extraction subunit 601212, configured to extract an intensity of a second characteristic peak corresponding to the second characteristic component;
the calculation unit 60122 includes:
a calculation subunit 601221, configured to calculate, according to the intensity of the first characteristic peak and the intensity of the second characteristic peak, a ratio of the intensities of the first characteristic peak and the second characteristic peak, and output the ratio as the exposure index E.
Optionally, the evaluation unit 603 includes:
a first evaluation subunit 6031 configured to determine, according to the evaluation strategy and the exposure index E, a first evaluation result of the coating completeness of the shell-core structure material corresponding to a value of the exposure index E;
a second evaluation subunit 6032 configured to determine, according to the evaluation strategy and the electrical conductivity of the shell-core structural material, a second evaluation result of the coating completeness of the shell-core structural material corresponding to a value of the electrical conductivity of the shell-core structural material;
a determination unit 6033 configured to compare the first evaluation result with the second evaluation result, and if the first evaluation result matches the second evaluation result, output the evaluation result as an evaluation result of the coating completeness of the core-shell structure material.
Specifically, the shell-core structure material is Si @ C, the first characteristic component is Si, and the second characteristic component is C; the first evaluation subunit respectively acquires Si with wave number of 500cm according to the Raman spectrum of the Si @ C-1The peak intensity of C at a wave number of 1580cm-1(ii) peak intensity of; the exposure index E is that the Si is 500cm-1(ii) peak intensity of (D) and said C at wave number of 1580cm-1The smaller the value of the exposure index E, the higher the coating completeness of the core-shell structured material.
Fig. 7 is a block diagram of a test apparatus 700 for testing the completeness of coating of a li-ion battery shell core structure material according to an exemplary embodiment of the invention.
As shown in fig. 7, the test apparatus 700 includes:
a memory 701, a processor 702, and a computer program stored in the memory 701 and executable on the processor 502; the processor 702 is configured to implement the method for evaluating the coating completeness of the lithium ion battery core-shell structure material described in the above embodiments when executing the computer program.
The invention further provides a computer-readable storage medium, which stores a computer program, and when the computer program is executed by a processor, the method for evaluating the coating completeness of the lithium ion battery shell-core structure material described in the above embodiments is implemented.
To sum up:
the embodiment of the invention provides an evaluation method for coating completeness of a lithium ion battery shell-core structure material, solves the problem that only a microscopic representation means can be adopted in the existing battery material coating inspection, has the characteristics of simplicity, convenience and high efficiency while ensuring the accuracy, can reflect the overall coating state of the material, and has important significance for shortening the overall research and development test period and improving the screening efficiency of excellent and defective products.
As will be appreciated by one skilled in the art, embodiments of the present invention may be provided as a method, system, or computer program product. Accordingly, the present invention may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects. Furthermore, the present invention may take the form of a computer program product embodied on one or more computer-usable storage media (including, but not limited to, disk storage, optical storage, and the like) having computer-usable program code embodied therein.
The present invention is described with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems), and computer program products according to embodiments of the invention. It will be understood that each flow and/or block of the flow diagrams and/or block diagrams, and combinations of flows and/or blocks in the flow diagrams and/or block diagrams, can be implemented by computer program instructions. These computer program instructions may be provided to a processor of a general purpose computer, special purpose computer, embedded processor, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions specified in the flowchart flow or flows and/or block diagram block or blocks.
These computer program instructions may also be stored in a computer-readable memory that can direct a computer or other programmable data processing apparatus to function in a particular manner, such that the instructions stored in the computer-readable memory produce an article of manufacture including instruction means which implement the function specified in the flowchart flow or flows and/or block diagram block or blocks.
These computer program instructions may also be loaded onto a computer or other programmable data processing apparatus to cause a series of operational steps to be performed on the computer or other programmable apparatus to produce a computer implemented process such that the instructions which execute on the computer or other programmable apparatus provide steps for implementing the functions specified in the flowchart flow or flows and/or block diagram block or blocks.
It is to be understood that the present invention is not limited to the procedures and structures described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (15)
1. A method for evaluating the coating completeness of a shell-core structure material of a lithium ion battery is characterized by comprising the following steps:
respectively carrying out Raman spectrum detection and conductivity detection on the shell-core structure material; the shell-core structure material is formed by compounding an inner layer and an outer layer, and the outer layer is completely coated on the inner layer; the coating completeness is used for determining whether the outer layer of the shell-core structure material is completely coated on the inner layer material;
and obtaining the evaluation result of the coating completeness of the shell-core structure material according to the results of the Raman spectrum detection and the conductivity detection.
2. The evaluation method of claim 1, wherein the Raman mapping assay comprises:
obtaining a Raman spectrum of the shell-core structure material;
analyzing the Raman spectrum of the shell-core structure material to determine an exposure index E;
the obtaining of the evaluation result of the coating completeness of the shell-core structure material comprises:
and determining the evaluation result of the coating completeness of the shell-core structure material according to the exposure index E and the conductivity.
3. The method of claim 2, wherein the core-shell structural material comprises an inner layer and an outer layer, and the exposure index E corresponds to the completeness of coating of the inner layer by the outer layer; the operation of analyzing the Raman spectrum of the core-shell structure material and determining the exposure index E specifically comprises the following steps:
extracting the intensity of at least one characteristic peak of each characteristic component from the Raman spectrum of the core-shell structure material according to the at least one characteristic component of the inner layer and the outer layer respectively;
calculating the exposure index E based on the intensity of at least one characteristic peak of each of the characteristic components.
4. The method of claim 3, wherein the inner layer of the core-shell structural material comprises a first characteristic component and the outer layer comprises a second characteristic component; extracting the intensity of a first characteristic peak corresponding to the first characteristic component, and extracting the intensity of a second characteristic peak corresponding to the second characteristic component;
said operation of calculating said exposure index E based on the intensity of at least one characteristic peak of each of said characteristic components comprises:
and calculating the ratio of the intensities of the first characteristic peak and the second characteristic peak according to the intensity of the first characteristic peak and the intensity of the second characteristic peak, and outputting the ratio as the exposure index E.
5. The evaluation method according to claim 3, wherein the evaluation result of the coating completeness of the core-shell structure material is obtained according to the exposure index E, the conductivity of the core-shell structure material and a preset evaluation strategy, and the process specifically comprises:
determining a first evaluation result of the coating completeness of the shell-core structural material corresponding to the value of the exposure index E according to the evaluation strategy and the exposure index E;
determining a second evaluation result of the coating completeness of the shell-core structural material corresponding to the value of the conductivity of the shell-core structural material according to the evaluation strategy and the conductivity of the shell-core structural material;
and if the first evaluation result is consistent with the second evaluation result, outputting the evaluation result as the evaluation result of the coating completeness of the shell-core structure material.
6. The evaluation method according to claim 4, wherein the core-shell structural material is silicon Si @ carbon C, the first characteristic component is Si, and the second characteristic component is C; obtaining the wave number of Si at 500cm according to the Raman spectrum of the Si @ C-1The peak intensity of C at a wave number of 1580cm-1(ii) peak intensity of; the exposure index E is that the Si is 500cm-1(ii) peak intensity of (D) and said C at wave number of 1580cm-1The ratio of peak intensities of (a).
7. The evaluation method of any one of claims 1 to 6, further comprising, prior to performing the Raman spectrum detection and the conductivity detection:
purifying the shell-core structure material to remove impurities in the shell-core structure material.
8. A test device for the coating completeness of a lithium ion battery shell and core structure material is characterized by comprising:
the first testing unit is used for carrying out Raman spectrum detection on the shell-core structure material;
the second test unit is used for detecting the conductivity of the shell-core structure material;
and the evaluation unit is used for acquiring the evaluation result of the coating completeness of the shell-core structure material according to the detection results of the first test unit and the second test unit.
9. The test apparatus of claim 8, wherein the first test unit comprises:
the acquisition unit is used for acquiring a Raman spectrum of the shell-core structure material;
and the analysis unit is used for analyzing the Raman spectrum of the core-shell structure material and determining the exposure index E.
10. The test device of claim 9, wherein the core-shell structural material comprises an inner layer and an outer layer, the exposure index E corresponding to the completeness of coating of the inner layer by the outer layer; the analysis unit includes:
an extraction unit, which is used for extracting the intensity of at least one characteristic peak of each characteristic component from the Raman spectrum of the shell-core structure material according to the at least one characteristic component of the inner layer and the outer layer;
and the calculation unit is used for calculating the exposure index E according to the intensity of at least one characteristic peak of each characteristic component.
11. The test device of claim 10, wherein the inner layer of the core-shell structural material comprises a first characteristic component and the outer layer comprises a second characteristic component; the extraction unit includes:
a first extraction subunit configured to extract an intensity of a first characteristic peak corresponding to the first characteristic component;
a second extraction subunit operable to extract an intensity of a second characteristic peak corresponding to the second characteristic component;
the calculation unit includes:
and a calculating subunit, configured to calculate, based on the intensity of the first characteristic peak and the intensity of the second characteristic peak, a ratio of the intensities of the first characteristic peak and the second characteristic peak, which is output as the exposure index E.
12. The test device of claim 10, wherein the evaluation unit comprises:
a first evaluation subunit, configured to determine, according to an evaluation strategy and the exposure index E, a first evaluation result of the coating completeness of the core-shell structured material corresponding to the value of the exposure index E;
a second evaluation subunit, configured to determine, according to an evaluation strategy and the electrical conductivity of the shell-core structure material, a second evaluation result of the coating completeness of the shell-core structure material corresponding to the value of the electrical conductivity of the shell-core structure material;
and a judging unit for comparing the first evaluation result with the second evaluation result, and outputting the evaluation result as an evaluation result of the coating completeness of the core-shell structure material if the first evaluation result is consistent with the second evaluation result.
13. The device of claim 12, wherein the core-shell structural material is Si @ C, the first characteristic component is Si, and the second characteristic component is C; the first evaluation subunit respectively acquires Si with wave number of 500cm according to the Raman spectrum of the Si @ C-1The peak intensity of C at a wave number of 1580cm-1(ii) peak intensity of; the exposure index E is that the Si is 500cm-1(ii) peak intensity of (D) and said C at wave number of 1580cm-1The ratio of peak intensities of (a).
14. A test device for the coating completeness of a lithium ion battery shell and core structure material is characterized by comprising:
a memory, a processor, and a computer program stored in the memory and executable on the processor; wherein the processor is configured to implement the method for evaluating the coating completeness of the lithium ion battery shell and core structure material according to any one of claims 1 to 7 when executing the computer program.
15. A computer-readable storage medium, characterized in that the computer-readable storage medium stores a computer program, and the computer program is executed by a processor to implement the method for evaluating the coating completeness of the lithium ion battery shell and core structure material according to any one of claims 1 to 7.
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